Water → HCID 59860533、化合物

HRID 1877329ノート

反応式

HRID 1877329 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][CH:6]2O.C1(P([N:26]=[N+:27]=[N-:28])(C2C=CC=CC=2)=O)C=CC=CC=1.N12CCCN=C1CCCCC2.O>C1COCC1>[N:26]([CH:6]1[C:7]2[C:3](=[C:2]([CH3:1])[CH:10]=[CH:9][CH:8]=2)[CH2:4][CH2:5]1)=[N+:27]=[N-:28]

参加物

6

反応物 4

HCID 962WaterHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 199401P,P-Diphenylphosphinic azideHCID 109863964-methyl-2,3-dihydro-1H-inden-1-ol

生成物 1

HCID 59860533HCID 59860533、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4.34 g (29.28 mmol) 4-methyl-indan-1-ol and 7.8 ml (35.14 mmol) diphenylphosphoryl azide are dissolved in dry THF at room temperature under argon. To this mixture is added slowly 5.0 ml (35.14 mmol) 1,8-diazabicyclo[5.4.0]undec-7-ene. The reaction is stirred for 6 h at room temperature (TLC monitoring). Then the mixture is poured into water and extracted three times with toluene. The organic layers are combined, dried over MgSO4 and concentrated in vacuo. Purification using silica gel chromatography (hexane/EtOAc 9:1) affords pure 1-azido-4-methyl-indane as light orange liquid.

後処理

  1. extractionextracted three times with toluene
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customPurification

出典と根拠

ORDレコード
ord-4e338ed61eac4779b1a3a29a2f55bae5
出典データセット
uspto-grants-2012_11
特許番号
US08309739B2

反応ノート

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